CN111013524A - Synthesis device and synthesis method of iron oxide magnetic nano material - Google Patents
Synthesis device and synthesis method of iron oxide magnetic nano material Download PDFInfo
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- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 59
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 45
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 28
- 238000001308 synthesis method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 69
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 47
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- 239000002105 nanoparticle Substances 0.000 claims description 35
- 239000002244 precipitate Substances 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 29
- 239000001301 oxygen Substances 0.000 claims description 29
- 229910052760 oxygen Inorganic materials 0.000 claims description 29
- 239000011261 inert gas Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- 238000007789 sealing Methods 0.000 claims description 18
- 238000007885 magnetic separation Methods 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 16
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 13
- 229910001447 ferric ion Inorganic materials 0.000 claims description 13
- -1 polyethylene Polymers 0.000 claims description 13
- 229920000573 polyethylene Polymers 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
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- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000002505 iron Chemical class 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
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- 230000000694 effects Effects 0.000 description 10
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- 238000006460 hydrolysis reaction Methods 0.000 description 10
- 235000013980 iron oxide Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
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- 150000004677 hydrates Chemical class 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
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- 230000004044 response Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
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- 229940032296 ferric chloride Drugs 0.000 description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 2
- 229960002089 ferrous chloride Drugs 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical group Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 description 1
- 210000003292 kidney cell Anatomy 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
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- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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Abstract
The invention relates to a synthesis device and a synthesis method of iron oxide magnetic nano materials, and the technical scheme is that a water bath is placed on a supporting plate of a constant-temperature magnetic stirrer, water is filled in a cavity of the water bath, the lower part of a three-neck round-bottom flask is soaked in the water, an air inlet of a vacuum pump is connected with a first connector of a tee joint through a first hose, an air outlet of an air bag is connected with a second connector of the tee joint through a second hose, a third connector of the tee joint is hermetically connected with one inlet and outlet of the three-neck round-bottom flask through a third hose, and the other two inlets and outlets of the three-neck round-bottom flask are respectively provided with aThe device can flexibly control the multiphase reaction process of nano synthesis through the device, reasonably regulates and optimizes the influencing factors of coprecipitation reaction, and ensures that the synthesized magnetic nano Fe is obtained by controlling the synthesis conditions3O4And nano α -Fe2O3Good monodispersity, controllable particle size, high purity and controllable form.
Description
Technical Field
The invention belongs to the field of inorganic nano material synthesis, and relates to a synthesis device and a synthesis method of an iron oxide magnetic nano material.
Background
The magnetic nanoparticles are superfine magnetic materials with at least one dimension in the three-dimensional dimension of nano scale (1-100 nm), have the characteristics of small size, large specific surface area, high activity and the like of common nano materials, and have the characteristics of superparamagnetism and the like, and are novel materials. Due to nanoscale iron oxides (nano-Fe)3O4Nanometer α -Fe2O3Etc.) has the advantages of higher reactivity, easy separation, high reactivity and the like, is widely applied to various fields of biomedicine, environmental remediation, wastewater treatment and the like, becomes a class of nano materials which are widely applied, and is one of the hotspots of material research.
Wherein the nanometer is α -Fe2O3The n-type semiconductor with band gap is the most stable ferrite, has the characteristics of high catalytic activity, low production cost, strong corrosion resistance, semiconductor property, small environmental pollution and the like, and has a great number of applications in inorganic pigments, magnetic materials, photosensitive catalysts, environmental protection, medicine and biological engineering, such as rod-shaped and spindle-shaped nanometer α -Fe2O3Has higher remanent magnetization and coercive force, and the hollow spherical nanometer α -Fe2O3Based on the characteristics of small density, large specific surface area and the like, the spherical nano α -Fe particle with the particle size of about 10nm is mainly applied to the wastewater treatment process and the field of photoelectrocatalysis2O3The product has high chroma, high transparency and high tinting strength, and is widely applied to the fields of building coatings, rubber, plastics, printing ink, catalysts and the like. And nano Fe3O4Has the characteristics of relatively friendly environment, high reaction activity, easy modification and recovery and the like, and can be used for environment restoration treatment and medicineAnd bioengineering, for example: nano Fe3O4Due to the easy functionalization and superparamagnetic properties, they are commonly used in medical contrast agents and targeted drug delivery; and magnetic nano Fe3O4Due to the characteristics of large specific surface area, strong reactivity, easy recovery and the like, the metal oxide is widely used as a repairing agent for heavy metals and organic polluted water bodies, and particularly has good effect on adsorption of trace heavy metals in water. So that nano Fe3O4And nano α -Fe2O3Becoming one of the most important magnetic nanomaterials.
Nano Fe3O4And nano α -Fe2O3The synthesis method is diversified, and the selection of the method is based on the principles of stable and easily-controlled synthesis process, low synthesis cost, green and pollution-free preparation process, controllable particle size of finished products and the like. Common synthetic methods mainly comprise the following types:
(1) thermal decomposition method
The thermal decomposition method comprises adding organic precursor containing iron into hot solution containing surfactant, decomposing at high temperature to generate iron atom, and further oxidizing the iron atom to generate nanometer Fe3O4And nano α -Fe2O3. The thermal decomposition method has the advantages of controllable particle size, narrow particle size distribution, good dispersibility and the like, but the thermal decomposition method has the disadvantages of large energy consumption, complicated steps and high reaction temperature, and simultaneously uses a large amount of toxic and harmful organic chemical reagents, is not a green synthesis technology and has potential risks to the environment.
(2) Microemulsion process
The microemulsion method is nano Fe3O4The important synthesis method of the nano-particle utilizes the oil-water mixture to synthesize the nano-particle under the action of the surfactant, and has the advantages of good monodispersity and interface property of the nano-particle. But compared with other methods, the method has the defects of low yield, narrow application range and the like, the cleaning step of the material after the synthesis reaction is more complicated, and the by-product generated in the synthesis process is easy to cause environmental pollution.
(3) Coprecipitation method
The coprecipitation method isPreparation of nano-Fe by salt solution3O4The classical method has the characteristics of simplicity and effectiveness. The principle is that under the protection of inert gas, Fe in iron salt is caused to be in an alkaline environment2+And Fe3+Through oxidation-reduction reaction and coprecipitation, nano Fe is obtained3O4. The factors such as reaction temperature, pH value, alkali liquor type, mixing speed, medium ionic strength, iron salt addition sequence and the like can influence the nano Fe3O4Particle size and magnetic properties.
The whole reaction formula is as follows:
Fe2++2Fe3++8OH-→Fe3O4↓+4H2O
the coprecipitation method has the advantages of no secondary pollution and simple synthesis method, but the traditional coprecipitation method needs to be continuously introduced with inert gas (such as nitrogen) for protection, and the installation of a protective gas device is complicated and heavy, thereby causing the cost to be increased.
(4) Hydrothermal or solvent synthesis
Nano Fe3O4And nano α -Fe2O3The hydrothermal method or the solvent synthesis method is to synthesize the nano Fe in the solution under the high-temperature high-pressure reaction condition3O4And nano α -Fe2O3The nano-particles have the advantages of regular shape, uniform particle size distribution, good magnetic response and the like. The disadvantages are long reaction time, high requirement on equipment, secondary pollution caused by adding an organic reducing agent in the reaction, high production cost, and no contribution to large-scale industrial production and small-amount rapid synthesis in a laboratory.
(5) Template method
The template method is mainly used for nano α -Fe2O3The synthesis of the nano α -Fe is a synthesis method which takes a template as a main body configuration to control, influence and modify the shape and the size of a material and further determine the property of the material2O3The preparation method mainly adopts anode alumina, carbon nano-tubes, carbon microspheres, porous silica and the like as templates, and the template method can prepare the nano α -Fe with specific shape and structure2O3However, reaction by template methodThe method has low speed, the template needs to be washed by alkali liquor after synthesis, the operation is complicated, the cost is increased, the washed alkali liquor containing silicon and aluminum also causes certain pollution, and the method is not an environment-friendly synthesis method and does not utilize control cost.
(5) High temperature gas phase process
The high-temperature gas phase method mainly comprises a high-temperature evaporation condensation method, a chemical vapor deposition method and a laser ablation method, wherein the chemical vapor deposition method is mainly used and comprises an in-situ thermal oxidation method and a metal organic chemical vapor deposition method, the so-called in-situ thermal oxidation method is to oxidize a high-purity iron sheet at a high temperature by using a small amount of water vapor or oxygen to grow nano α -Fe in situ2O3A ribbon or a pellet of (a).
(6) Forced hydrolysis method
The forced hydrolysis method is an important method for preparing monodisperse nano particles by utilizing forced hydrolysis of metal salt solution and is used for synthesizing nano α -Fe2O3The method is particularly important, the forced hydrolysis method is simple to operate, mild in condition and good in performance of the obtained particles, and can be used for producing the nano particles in batches, and the principle of the forced hydrolysis method is as follows: fe3+Hydrolysis to yield Fe (OH)3Recrystallization to α -Fe2O3。Fe3+→Fe(OH)3→α-Fe2O3However, the forced hydrolysis method has long micro-mixing time, and the synthesis process may not have sufficient oxidation, so that the purity of the synthesized nano material is not high.
The invention aims at solving the technical problem of nano Fe3O4The defects and problems of the existing synthesis method comprise the defects of complicated synthesis steps, harsh synthesis conditions, low crystallization purity, expensive synthesis device, environmental pollution caused by synthesis byproducts, low efficiency in the separation and washing process (such as common precipitation method or centrifugal method, low efficiency and complicated operation) and the like.
Therefore, the synthesis method and the device which are simple and effective in development, low in cost, environment-friendly and wide in applicability are used for preparing the nano Fe with controllable particle size, controllable form, high purity and good monodispersity3O4And nano α -Fe2O3Is a research subject to be solved urgently at present.
Disclosure of Invention
In view of the above situation, the present invention aims to overcome the defects of the prior art and provide a method for synthesizing nano Fe3O4And nano α -Fe2O3And synthesizing nano Fe3O4And nano α -Fe2O3To realize the nano Fe3O4Or nano α -Fe2O3Low cost, no pollution and controllable synthesis.
The technical scheme of the invention is as follows:
a device for synthesizing iron oxide magnetic nano materials comprises a three-neck round-bottom flask, a water bath, a constant-temperature magnetic stirrer, a vacuum pump and an air bag, wherein the water bath is placed on a supporting plate of the constant-temperature magnetic stirrer, water is filled in a cavity of the water bath, the lower part of the three-neck round-bottom flask is soaked in the water, an air inlet of the vacuum pump is connected with a first connector of a tee joint through a first hose, an air outlet of the air bag is connected with a second connector of the tee joint through a second hose, a third connector of the tee joint is in sealing connection with one inlet and one outlet of the three-neck round-bottom flask through a third hose, a burette and a separating funnel which are in sealing connection are respectively arranged on the other two inlets and the other two outlets of the three-neck round-bottom flask, a first valve is arranged on the first hose, a second valve is arranged on the.
Preferably, the three exit of three neck round flask on be equipped with the rubber buffer respectively, the rubber buffer center is opened has the feedstock channel who link up from top to bottom, buret and separating funnel's discharge end arrange in feedstock channel and closely laminate with the rubber buffer inner wall, constitute three neck round flask's sealed feeding structure.
Preferably, the third hose is equipped with the joint intubate with three-neck round flask import and export sealing connection's one end, and the discharge end of joint intubate is arranged in charge-in channel and is closely laminated with the rubber buffer inner wall, constitutes three-neck round flask's sealed gas business turn over passageway structure.
Preferably, the constant-temperature magnetic stirrer is placed on a workbench, a positioning support is further arranged on the workbench, and a fixing clamp used for fixing the positions of the three-neck round-bottom flask, the burette and the separating funnel is arranged on the positioning support.
Preferably, the workbench is further provided with a drying and collecting device for drying and collecting the iron oxide magnetic nano material, and the drying and collecting device comprises a polyethylene bottle, a magnet and a constant-temperature drying box.
Preferably, the gas bag is filled with inert gas as nano Fe3O4The protective gas or the air bag of the synthetic reaction is filled with high-purity oxygen which is used as nanometer α -Fe2O3Protective gas for the synthesis reaction.
Preferably, the water bath is provided with a thermometer for monitoring the temperature of the water.
Adopt above-mentioned synthesizer's nanometer Fe3O4The synthesis method comprises the following steps:
(1) nano Fe3O4Synthesis of (2)
Closing the first valve, the second valve and the third valve, connecting the air bag filled with inert gas with a second hose, dissolving ferrous salt and ferric salt with ultrapure water to obtain a mixed solution, wherein Fe in the mixed solution2+And Fe3+The molar ratio of the mixture to the liquid is 1:2, adding the mixed liquid into a separating funnel, simultaneously closing a valve of the separating funnel, hermetically connecting an outlet of the separating funnel with one inlet and outlet of a three-neck round-bottom flask, adding an alkaline liquid into a burette, simultaneously closing the valve of the burette, hermetically connecting an outlet of the burette with the other inlet and outlet of the three-neck round-bottom flask, opening the valve of the separating funnel, adding the mixed liquid in the separating funnel into the three-neck round-bottom flask, closing the valve of the separating funnel, hermetically connecting a third hose with the last inlet and outlet of the three-neck round-bottom flask, opening the first valve and the third valve to enable the first hose and the third hose to be communicated, sealing the second hose, opening a vacuum pump, exhausting air in the three-neck round-bottom flask until the pumping pressure of the vacuum pump is not changed, to show thatThe hose, the third hose and the three-neck round-bottom flask are in a vacuum state, the first valve is closed, the second valve is opened, the second hose and the third hose are communicated, the first hose is closed, the inner cavity of the three-neck round-bottom flask is automatically filled with inert gas in the gas bag through the second hose and the third hose under the action of negative pressure of the inert gas, the third valve is closed when the volume of the gas bag is not changed any more, and at the moment, the reaction space in the three-neck round-bottom flask is filled with the inert gas, so that the reaction process is ensured to be completed under the inert gas environment;
opening the constant-temperature magnetic stirrer, adjusting the temperature of the constant-temperature magnetic stirrer, heating the mixed solution to 80 ℃ through water constant-temperature water bath in the water bath, opening a rotor of the constant-temperature magnetic stirrer to stir continuously, opening a valve of the burette, adding alkaline liquid, controlling the pH value of the mixed solution to be between 8.0 and 14, carrying out constant-temperature reaction for about 40min, finishing the reaction, and cooling to obtain Fe3O4A nanoparticle suspension;
(2) cleaning, drying and collecting
Fe to be synthesized3O4Carrying out magnetic separation on the nanoparticle suspension, and removing the supernatant to obtain a precipitate; then washing the precipitate with methanol and ultrapure water respectively until the pH of the precipitate is neutral, and drying the precipitate to obtain the nano Fe3O4。
Nano α -Fe adopting synthesis device2O3The synthesis method comprises the following steps:
(1) nanometer α -Fe2O3Synthesis of (2)
Closing the first valve, the second valve and the third valve, connecting an air bag filled with high-purity oxygen with a second hose, adding pure water or a trivalent iron salt solution into the three-neck round-bottom flask through an inlet and an outlet of the three-neck round-bottom flask, adding the trivalent iron salt solution into the separating funnel, simultaneously closing the valve of the separating funnel, hermetically connecting an outlet of the separating funnel with one inlet and one outlet of the three-neck round-bottom flask, adding concentrated hydrochloric acid into the burette, simultaneously closing the valve of the burette, hermetically connecting an outlet of the burette with the other inlet and the other outlet of the three-neck round-bottom flask, hermetically connecting a third hose with the last inlet and the last outlet of the three-neck round-bottom flask, opening the first valve and the third valve to conduct the first hose and the third hose, sealing the second hose, opening a vacuum pump to exhaust air in the three-neck flask, until the pump pressure of the vacuum pump is not changed any more, the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, the first valve is closed, the second valve is opened, the second hose and the third hose are communicated, the first hose is closed, the inner cavity of the three-neck round-bottom flask is automatically filled with high-purity oxygen through the second hose and the third hose under the action of negative pressure of the high-purity oxygen in the air bag, the third valve is closed when the volume of the air bag is not changed any more, and the reaction space in the three-neck round-bottom flask is filled with the high-purity oxygen at the moment, so that the reaction process is finished under the high-purity oxygen environment;
opening a constant-temperature magnetic stirrer, adjusting the temperature of the constant-temperature magnetic stirrer, heating pure water or a trivalent ferric salt solution in a three-neck round-bottom flask to 90-100 ℃ through a water constant-temperature water bath in a water bath tub, opening a valve of a burette, adding concentrated hydrochloric acid, opening a rotor of the constant-temperature magnetic stirrer to continuously stir, simultaneously opening a valve of a separating funnel, adding the trivalent ferric salt solution, and enabling Fe in the three-neck round-bottom flask to be in Fe concentration3+The molar concentration ratio of the hydrochloric acid to the hydrochloric acid is 2:1-10:1, the pH value is controlled to be 1.0-3.0, a valve of a burette and a valve of a separating funnel are closed, stirring is carried out until trivalent ferric salt is completely dissolved, then the sealed three-neck round-bottom flask is placed into a constant temperature drying box at 100 ℃, the constant temperature is kept for 24-48 hours, and the synthesis is completed to obtain α -Fe2O3A nanoparticle suspension;
(2) cleaning, drying and collecting
The synthesized α -Fe2O3Magnetically separating the suspension of nanoparticles, removing the supernatant to obtain precipitate, repeatedly washing the precipitate with distilled water until chloride-free precipitate is obtained, and drying to obtain α -Fe nanoparticles2O3。
Compared with the prior art, the invention has the following advantages:
(1) combining co-precipitation and forced hydrolysis methods have similar synthesis conditions, including synthesis conditionsThe magnetic nano Fe-based catalyst has the characteristics of milder (high temperature and high pressure are not needed), reaction is completed under the conditions of closed environment and stirring in aqueous solution, and the like, and one set of equipment can be simultaneously suitable for magnetic nano Fe3O4And nano α -Fe2O3The structure is simple and easy to obtain, the operation of the synthetic process is simple, the synthetic conditions are controllable, and no by-product polluting the environment is generated in the synthetic process; realizes the nano Fe3O4Or nano α -Fe2O3The cost is low, no pollution is caused, and the controllable synthesis is realized;
(2) the device can flexibly control the multiphase reaction process of nano synthesis, reasonably regulate and optimize the influencing factors of coprecipitation reaction, and control the synthesis conditions to synthesize magnetic nano Fe3O4And nano α -Fe2O3The monodispersity is good, the particle size is controllable, the purity is high, and the form is controllable;
(3) the cytotoxicity experiment shows that the synthesized nano-particles have good biocompatibility;
(4) the synthetic product can be magnetic nano Fe by magnetic separation and enrichment technology3O4And nano α -Fe2O3The magnetic separation and enrichment recovery speed is high, and the nano Fe is separated from the solution3O4And nano α -Fe2O3Only 3-5 s are needed, and the recovery rate reaches 99%;
(5) the device can be suitable for various chemical reactions in reductive and oxidative environments, namely the change of the reaction environment can be realized by changing the types of gases (nitrogen, helium, oxygen and the like) in the air bag, and continuous introduction of protective gas is not needed, so that the device is complex and the cost is high. Due to the plurality of medicine adding openings, the medicine adding sequence and time can be flexibly controlled. Simple operation, convenient assembly and carrying, strong operability, low cost and wide application range.
(6) Can be in nano Fe by vacuumizing and air bag3O4Effectively removing oxygen in the reaction cavity in the synthesis process to ensure that the reaction process is finished under the inert gas environment, if the oxygen in the solution cannot be effectively removed in the reaction process, not only can the oxygen in the solution be effectively removedThe purity of the final product is influenced, and even the dissolved oxygen in the solution can generate nano Fe3O4Conversion to nano Fe2O3Thereby improving the purity of the product, and also producing the nano α -Fe2O3The reaction process can not ensure complete oxidation environment, and the nano α -Fe is synthesized2O3The product purity is not high in the process, and part of Fe is generated3O4Etc. occur. The device and the method provided by the invention are ensured to be carried out in a protective gas environment, and the purity of the product is improved.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
Figure 2 is an enlarged partial cross-sectional view of a three-neck round bottom flask of the present invention.
FIG. 3 shows the synthesis of nano-Fe in example 13O4Wherein the ordinate is the peak response intensity, the abscissa 2 theta is the angle of the product crystal lattice, and the characteristic peak of the product is synthesized with Fe3O4Comparison of standard cards revealed that the synthesized nanoparticles were Fe3O4；
FIG. 4 shows the nano Fe synthesized in example 13O4An electron microscope image;
FIG. 5 shows the synthesis of α -Fe nanoparticles from example 22O3XRD diffraction pattern of (including granular and rice-grain nano α -Fe)2O3Testing after mixing) wherein the ordinate is the peak response intensity and the abscissa 2 theta is the angle of the product lattice, by synthesizing the characteristic peak of the product with Fe2O3Comparing standard cards to obtain the synthesized nano Fe2O3Is α -Fe2O3A crystalline form;
FIG. 6 shows the synthesis of α -Fe nanoparticles from example 22O3In an electron microscope picture, the nano particles are round and granular, and the diameter of the particles is about 80 nm;
FIG. 7 shows rice-grain α -Fe of example 32O3An electron microscope image;
fig. 8 shows the result of cytotoxicity test of each nanomaterial.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples.
As shown in the figure 1-2, the device for synthesizing the iron oxide magnetic nano material comprises a three-neck round-bottom flask 6, a water bath 10, a constant-temperature magnetic stirrer 11, a vacuum pump 1 and an air bag 2, wherein the water bath 10 is placed on a supporting plate of the constant-temperature magnetic stirrer 11, water 10a is filled in a cavity of the water bath 10, the lower part of the three-neck round-bottom flask 6 is soaked in the water, an air inlet of the vacuum pump 1 is connected with a first connector of a tee joint 5 through a first hose 3a, an air outlet of the air bag 2 is connected with a second connector of the tee joint 5 through a second hose 3b, a third connector of the tee joint is connected with one inlet and outlet of the three-neck round-bottom flask 6 through a third hose 3c in a sealing manner, a burette 8 and a separating funnel 9 which are connected in a sealing manner are respectively arranged on the other two inlets and outlets of the three-neck round-bottom flask 6, a, a second valve 4b is arranged on the second hose 3b, and a third valve 4c is arranged on the third hose 3 c.
In order to ensure the using effect, the three ports 61 of the three-neck round-bottom flask 6 are respectively provided with a rubber plug 62, the center of the rubber plug 62 is provided with a feeding channel 62a which is through from top to bottom, the discharge ends of the burette 8 and the separating funnel 9 are arranged in the feeding channel 62a and tightly attached to the inner wall of the rubber plug, thus forming a sealed feeding structure of the three-neck round-bottom flask.
The one end of third hose 3c and three neck round bottom flask 6 import and export sealing connection is equipped with and connects intubate 7, connects the discharge end of intubate 7 and arranges in charge-in channel 62a and closely laminate with the rubber buffer inner wall in, constitutes the sealed gas business turn over passageway structure of three neck round bottom flasks.
The constant-temperature magnetic stirrer 11 is placed on a workbench 17, a positioning support 15 is further arranged on the workbench 17, a fixing clamp 16 for fixing the positions of the three-necked round-bottomed flask 6, the burette 8 and the separating funnel 9 is arranged on the positioning support, the purpose is to stabilize the positions of the three-necked round-bottomed flask 6, the burette 8 and the separating funnel 9 in the resynthesis process, the positioning support 15 and the fixing clamp 16 are in the prior art, for example, a conventional burette fixing frame can be adopted for fixing the burette and the separating funnel, the three-necked round-bottomed flask 6 can adopt a structure shown in figure 1 and comprises a base and a vertical supporting rod arranged on the base, a positioning ring in sliding connection can be arranged on the vertical supporting rod, a telescopic rod is connected on the positioning ring, the fixing clamp is arranged at the free end of the telescopic rod, a screw is arranged on the positioning ring, and the vertical supporting rod can slide up, the adjusting screw is screwed down after the adjusting screw is in place, so that the positioning ring can be pressed and fixed, the height of the positioning ring is adjusted, the telescopic rod is sleeved together through the two coaxial sleeve sliding sleeves, the fixing clamp center is provided with the mounting hole corresponding to the inlet of the three-neck round-bottom flask, and the fixation of the three-neck round-bottom flask can be realized through the screw pressing fixation.
The workbench 17 is also provided with a drying and collecting device for drying and collecting the iron oxide magnetic nano material, and the drying and collecting device comprises a polyethylene bottle 12, a magnet 13 and a constant-temperature drying box 14.
The air bag 2 is filled with inert gas as nano Fe3O4The protective gas or the air bag of the synthetic reaction is filled with high-purity oxygen which is used as nanometer α -Fe2O3Protective gas for the synthesis reaction.
The burette 8 is a basic burette, and sodium hydroxide solution, potassium hydroxide solution or ammonia water is filled in the burette and is used as nano Fe3O4Alkaline liquid for synthesis reaction, or acid burette 8 filled with concentrated hydrochloric acid as nanometer α -Fe2O3The acidic liquid of the synthesis reaction.
The separating funnel 9 is filled with ferrous ion solution or ferric ion solution or the combination of the ferrous ion solution and the ferric ion solution.
The water bath 10 is provided with a thermometer 18 for monitoring the temperature of the water.
Adopt above-mentioned synthesizer's nanometer Fe3O4The synthesis method comprises the following steps:
(1) nano Fe3O4Synthesis of (2)
The first valve 4a, the second valve 4b and the third valve 4c are closed, and the gas bag filled with inert gas and the second hose are connected3b, dissolving ferrous salt and ferric salt by using ultrapure water to obtain a mixed solution, wherein Fe in the mixed solution2+And Fe3+The molar ratio of the mixture to the liquid is 1:2, adding the mixed liquid into a separating funnel 9, simultaneously closing a valve 9a of the separating funnel 9, hermetically connecting an outlet of the separating funnel 9 with one inlet and outlet of a three-neck round-bottom flask 6, wherein the burette is an alkaline burette, adding an alkaline liquid into the burette, simultaneously closing a valve 8a of a burette 8, hermetically connecting an outlet of the burette with the other inlet and outlet of the three-neck round-bottom flask 6, opening the valve 9a of the separating funnel 9, adding the mixed liquid in the separating funnel 9 into the three-neck round-bottom flask 6, closing the valve 9a of the separating funnel 9, hermetically connecting a third hose with the last inlet and outlet of the three-neck round-bottom flask 6, and opening a first valve 4a and a third valve 4c to enable the first hose and the third hose to be communicated and seal a second hose, opening the vacuum pump 1, exhausting air in the three-neck round-bottom flask 6 till the pump pressure of the vacuum pump is not changed any more, indicating that the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, closing the first valve 4a, opening the second valve 4b to enable the second hose and the third hose to be communicated, sealing the first hose, automatically filling the inner cavity of the three-neck round-bottom flask through the second hose and the third hose under the action of the inert gas negative pressure in the gas bag, closing the third valve 3c when the volume of the gas bag is not changed any more, filling the reaction space in the three-neck round-bottom flask with inert gas at the moment, and ensuring that the reaction process is finished under the inert gas environment;
opening the constant temperature magnetic stirrer 11, adjusting the temperature of the constant temperature magnetic stirrer 11, heating the mixed solution to 80 ℃ through the water constant temperature water bath in the water bath 10, opening the rotor of the constant temperature magnetic stirrer 11 to stir continuously (the rotor is arranged in a three-neck round bottom flask in advance), opening the valve 8a of the burette 8, adding alkaline liquid, controlling the pH value of the mixed solution to be between 8.0 and 14, carrying out constant temperature reaction for about 40min, completing the reaction, cooling to obtain Fe3O4A nanoparticle suspension;
(2) cleaning, drying and collecting
Fe to be synthesized3O4Nanoparticle suspensionsCarrying out magnetic separation on the floating liquid, and removing the supernatant to obtain a precipitate; then washing the precipitate with methanol and ultrapure water respectively until the pH of the precipitate is neutral, and drying the precipitate to obtain the nano Fe3O4。
The ferrous salt is ferrous chloride, ferrous sulfate and hydrates thereof, and the ferric salt is ferric chloride or hydrates of ferric chloride. Ferrous nitrate or ferric nitrate is avoided as much as possible, because nitric acid generated in the nitrate hydrolysis process has certain oxidizability and can lead Fe2+Is oxidized into Fe3+Resulting in the formation of Fe2O3Affecting the purity of the synthesized product. .
The alkaline liquid is any one of sodium hydroxide, potassium hydroxide and ammonia water.
The inert gas is nitrogen or helium.
Nano α -Fe adopting synthesis device2O3The synthesis method comprises the following steps:
(1) nanometer α -Fe2O3Synthesis of (2)
Closing a first valve 4a, a second valve 4b and a third valve 4c, connecting an air bag filled with high purity oxygen with a second hose 3b, adding pure water or a trivalent iron salt solution into the three-neck round-bottom flask through an inlet and an outlet of the three-neck round-bottom flask 6, adding the trivalent iron salt solution into a separating funnel 9, simultaneously closing a valve 9a of the separating funnel 9, hermetically connecting an outlet of the separating funnel 9 with one inlet and an outlet of the three-neck round-bottom flask 6, adding concentrated hydrochloric acid into a burette, simultaneously closing a valve 8a of a burette 8, hermetically connecting an outlet of the burette with the other inlet and the outlet of the three-neck round-bottom flask 6, hermetically connecting a third hose with the last inlet and the outlet of the three-neck round-bottom flask 6, and opening the first valve 4a and the third valve 4c when the three-neck round-bottom flask 6 is in a relatively closed environment, the first hose and the third hose are communicated, the second hose is closed, the vacuum pump 1 is opened, air in the three-neck round-bottom flask 6 is exhausted until the pump pressure of the vacuum pump is not changed any more, the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, the first valve 4a is closed, the second valve 4b is opened, the second hose and the third hose are communicated, the first hose is closed, the inner cavity of the three-neck round-bottom flask is automatically filled with the high-purity oxygen through the second hose and the third hose under the negative pressure action of the high-purity oxygen in the air bag, the third valve 3c is closed when the volume of the air bag is not changed any more, and at the moment, the reaction space in the three-neck round-bottom flask is filled with the high-purity oxygen, so that the reaction process is finished under the;
opening the constant temperature magnetic stirrer 11, adjusting the temperature of the constant temperature magnetic stirrer 11, heating the pure water in the three-neck round-bottom flask to 90-100 ℃ through the water constant temperature water bath in the water bath 10, opening the valve 8a of the burette 8, adding the concentrated hydrochloric acid, opening the rotor of the constant temperature magnetic stirrer 11 to stir continuously (the rotor is filled in the three-neck round-bottom flask in advance), simultaneously opening the valve 9a of the separating funnel 9, adding the trivalent ferric salt solution, and leading the Fe in the three-neck round-bottom flask to be Fe3+The molar concentration ratio of the solution to hydrochloric acid is 2:1-10:1, the pH value is controlled to be 1.0-3.0, because the proper initial concentration of hydrochloric acid is kept, the hydrolysis precipitation and crystallization growth speed can be reduced, so that the nano particles grow completely and uniformly, then a valve 8a of a burette 8 and a valve 9a of a separating funnel 9 are quickly closed, the stirring is carried out until the trivalent ferric salt is completely dissolved, then the closed three-neck round bottom flask is placed into a constant temperature drying box 14 at 100 ℃, the constant temperature is carried out for 24-48 h, the synthesis is completed, and α -Fe is obtained2O3A nanoparticle suspension;
(2) cleaning, drying and collecting
The synthesized α -Fe2O3Magnetically separating the suspension of nanoparticles, removing the supernatant to obtain precipitate, repeatedly washing the precipitate with distilled water until chloride-free precipitate is obtained, and drying to obtain α -Fe nanoparticles2O3。
The solution of the trivalent ferric salt is FeCl3And hydrates thereof.
Nano Fe3O4Synthetic method example 1:
(1) nano Fe3O4Synthesis of (2)
The first valve 4a, the second valve 4b and the third valve 4c are closed, and the gas bag filled with inert gas is filledConnected to the second tube 3b, 1g of ferrous chloride tetrahydrate and 2.7g of ferric chloride hexahydrate were dissolved in 50mL of ultrapure water in a beaker to obtain a mixed solution containing Fe2+And Fe3+The molar ratio of the mixture to the liquid is 1:2, adding the mixed liquid into a separating funnel 9, simultaneously closing a valve 9a of the separating funnel 9, hermetically connecting an outlet of the separating funnel 9 with one inlet and outlet of a three-neck round-bottom flask 6, wherein the burette is an alkaline burette, adding ammonia water with the concentration of 25% -28% into the burette, simultaneously closing a valve 8a of a burette 8, hermetically connecting an outlet of the burette with the other inlet and outlet of the three-neck round-bottom flask 6, opening the valve 9a of the separating funnel 9, adding the mixed liquid in the separating funnel 9 into the three-neck round-bottom flask 6, closing the valve 9a of the separating funnel 9, hermetically connecting a third hose with the last inlet and outlet of the three-neck round-bottom flask 6, and opening a first valve 4a and a third valve 4c to enable the first hose and the third hose to be communicated, the second hose is closed, the vacuum pump 1 is opened, air in the three-neck round-bottom flask 6 is exhausted until the pumping pressure of the vacuum pump is not changed any more, the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, the first valve 4a is closed, the second valve 4b is opened, the second hose and the third hose are communicated, the first hose is closed, the inner cavity of the three-neck round-bottom flask is automatically filled with inert gas through the second hose and the third hose under the action of the negative pressure of the inert gas in the gas bag, and the third valve 3c is closed when the volume of the gas bag is not changed any more, at the moment, the reaction space in the three-neck round-bottom flask is filled with the inert gas, so that the reaction process is guaranteed to be completed under the;
opening the constant-temperature magnetic stirrer 11, adjusting the temperature of the constant-temperature magnetic stirrer 11, heating the mixed solution to 80 ℃ through a water constant-temperature water bath in the water bath 10, opening a rotor of the constant-temperature magnetic stirrer 11 to stir continuously (the rotor is arranged in a three-neck round-bottom flask in advance), rotating at the speed of 150rpm, opening a valve 8a of the burette 8, uniformly adding 28mL of ammonia water, controlling the pH value of the mixed solution to be between 8 and 10, carrying out constant-temperature reaction for about 40min, completing the reaction, cooling to obtain Fe3O4A nanoparticle suspension;
the separating funnel 9 is taken down and the liquid is separated,pulling out the rubber stopper of the inlet and outlet of the three-neck round-bottom flask 6, and introducing the Fe obtained by the reaction through the inlet and outlet of the three-neck round-bottom flask 63O4Pouring the nanoparticle suspension into a polyethylene bottle 12, placing a magnet (neodymium iron boron magnet) at the bottom of the polyethylene bottle, performing magnetic separation, after about 4s, after the precipitate is gathered at the bottom of the polyethylene bottle to show that the magnetic separation is finished, discarding the supernatant to obtain a precipitate, adding methanol into the polyethylene bottle, performing vibration cleaning for 5min, performing magnetic separation by using the magnet, and discarding the supernatant; adding ultrapure water, ultrasonic cleaning for 5min, performing magnetic separation with magnet, discarding supernatant, repeatedly washing until the pH of precipitate is neutral, oven drying the obtained precipitate in constant temperature drying oven 14 at low temperature, and grinding to obtain nanometer Fe3O4。
The XRD spectrogram and electron micrograph of the obtained nanometer material are shown in figures 3 and 4, and the XRD spectrogram of figure 3 shows that the nanometer Fe3O4The purity is high, and the electron microscopic picture in figure 4 shows that the synthesized nano Fe3O4The magnetic separation is round and granular, the grain diameter is about 25nm, the dispersity is good, the magnetic separation time is about 3s, and the recovery rate reaches more than 99%.
Nanometer α -Fe2O3Synthetic method example 2:
(1) nanometer α -Fe2O3Synthesis of (2)
Closing a first valve 4a, a second valve 4b and a third valve 4c, connecting an air bag filled with high purity oxygen with a second hose 3b, adding pure water into the three-neck round-bottom flask through an inlet and an outlet of the three-neck round-bottom flask 6, adding a ferric iron salt solution into a separating funnel 9, wherein the ferric iron salt solution adopts a ferric trichloride hexahydrate solution, simultaneously closing a valve 9a of the separating funnel 9, connecting an outlet of the separating funnel 9 with one inlet and an outlet of the three-neck round-bottom flask 6 in a sealing manner, adding concentrated hydrochloric acid with the concentration of 37% into the burette, simultaneously closing a valve 8a of a burette 8, connecting an outlet of the burette with the other inlet and the outlet of the three-neck round-bottom flask 6 in a sealing manner, connecting the third hose with the last inlet and the outlet of the three-neck flask 6 in a sealing manner, and keeping the three-neck round-bottom flask 6 in a relatively sealed environment, opening a first valve 4a and a third valve 4c to enable the first hose and the third hose to be communicated, sealing a second hose, opening a vacuum pump 1 to exhaust air in the three-neck round-bottom flask 6 until the pump pressure of the vacuum pump is not changed any more, indicating that the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, closing the first valve 4a, opening a second valve 4b to enable the second hose and the third hose to be communicated, sealing the first hose, automatically filling the inner cavity of the three-neck round-bottom flask through the second hose and the third hose under the action of the negative pressure of high-purity oxygen in the air bag, closing the third valve 3c when the volume of the air bag is not changed any more, and at the moment, filling the reaction space in the three-neck round-bottom flask with high-purity oxygen to ensure that the reaction process is completed under the high-purity oxygen environment;
opening the constant temperature magnetic stirrer 11, adjusting the temperature of the constant temperature magnetic stirrer 11, heating the pure water in the three-neck round-bottom flask to 95 ℃ through the water constant temperature water bath in the water bath 10, opening the valve 8a of the burette 8, adding concentrated hydrochloric acid, opening the rotor of the constant temperature magnetic stirrer 11 to continuously stir at the rotating speed of 150rpm so that the concentration of hydrochloric acid reaches 0.002mol/L, simultaneously opening the valve 9a of the separating funnel 9, adding a trivalent ferric salt solution so as to obtain 0.02mol/L Fe in the three-neck round-bottom flask3+Solution of Fe3+The molar concentration ratio of the solution to hydrochloric acid is 10:1, a valve 8a of a burette 8 and a valve 9a of a separating funnel 9 are quickly closed, the mixture is stirred until the trivalent ferric salt is completely dissolved, then the sealed three-neck round-bottom flask is placed into a constant temperature drying box 14 at 100 ℃, the constant temperature is kept for 24-48 h, and the synthesis is completed to obtain α -Fe2O3A nanoparticle suspension;
(2) cleaning, drying and collecting
α -Fe obtained by the reaction is introduced through the inlet and outlet of a three-neck round-bottom flask 62O3Pouring the nanoparticle suspension into polyethylene bottle 12, placing magnet (neodymium iron boron magnet) at the bottom of the polyethylene bottle, performing magnetic separation, collecting the precipitate at the bottom of the polyethylene bottle after about 4s, removing the supernatant to obtain precipitate, washing the precipitate with distilled water, performing magnetic separation with magnet, repeating the above steps until precipitate without chloride is obtained, oven drying the precipitate at 100 deg.C, and grinding to obtain nanometerα-Fe2O3。
The XRD spectrogram and electron micrograph of the obtained nanometer material are respectively shown in figures 5 and 6, and the XRD spectrogram of figure 5 shows that the synthesized nanometer Fe2O3Is α -Fe2O3Crystal form and high purity; as can be seen from the electron microscope image of FIG. 6, the synthesized particles are round particles, the particle diameter is about 80nm, and the magnetic separation process is about 4s, and the recovery rate reaches more than 99%.
Nanometer α -Fe2O3Synthetic method example 3:
(1) nanometer α -Fe2O3Synthesis of (2)
Closing the first valve 4a, the second valve 4b and the third valve 4c, connecting the air bag filled with high purity oxygen to the second hose 3b, and dissolving ferric chloride hexahydrate in pure water at room temperature to obtain 0.5mol/L Fe3+The solution is respectively added into a three-neck round-bottom flask and a separating funnel 9, a valve 9a of the separating funnel 9 is closed, an outlet of the separating funnel 9 is hermetically connected with one inlet and outlet of the three-neck round-bottom flask 6, a burette is an acid burette, concentrated hydrochloric acid with the concentration of 37% is added into the burette, a valve 8a of a burette 8 is closed, an outlet of the burette is hermetically connected with the other inlet and outlet of the three-neck round-bottom flask 6, a third hose is hermetically connected with the last inlet and outlet of the three-neck round-bottom flask 6, the three-neck round-bottom flask 6 is in a relatively airtight environment at the moment, a first valve 4a and a third valve 4c are opened, so that the first hose and the third hose are communicated, the second hose is closed, a vacuum pump 1 is opened, air in the three-neck round-bottom flask 6 is exhausted until the pump pressure of the vacuum pump is not changed any more, and the first hose, the third hose and the three-neck round-bottom flask are, closing the first valve 4a, opening the second valve 4b to enable the second hose and the third hose to be communicated, sealing the first hose, automatically filling the inner cavity of the three-neck round-bottom flask through the second hose and the third hose under the action of negative pressure of high-purity oxygen in the air bag, closing the third valve 3c when the volume of the air bag is not changed any more, filling high-purity oxygen in the reaction space in the three-neck round-bottom flask at the moment, and ensuring that the reaction process is finished under the high-purity oxygen environment;
opening the constant temperature magnetic stirrer 11, adjusting the temperature of the constant temperature magnetic stirrer 11, and heating Fe in the three-neck round-bottom flask through the water constant temperature water bath in the water bath 103+Opening a valve 8a of a burette 8 when the solution reaches 100 ℃, adding concentrated hydrochloric acid, opening a rotor of a constant-temperature magnetic stirrer 11 to stir continuously at the rotating speed of 150rpm so that the concentration of the hydrochloric acid reaches 0.025mol/L, simultaneously opening a valve 9a of a separating funnel 9, and adding Fe3+Solution of Fe in a three-necked round-bottomed flask3+The molar concentration ratio of the solution to hydrochloric acid is 2:1-10:1, the pH value is controlled to be 1.0-3.0, a valve 8a of a burette 8 and a valve 9a of a separating funnel 9 are quickly closed, stirring is carried out until trivalent ferric salt is completely dissolved, then a closed three-neck round bottom flask is placed into a constant temperature drying box 14 at 100 ℃, the constant temperature is kept for 36 hours, and the synthesis is finished to obtain α -Fe2O3A nanoparticle suspension;
(2) cleaning, drying and collecting
α -Fe obtained by the reaction is introduced through the inlet and outlet of a three-neck round-bottom flask 62O3Pouring the nanoparticle suspension into polyethylene bottle 12, placing magnet (neodymium iron boron magnet) at the bottom of the polyethylene bottle, performing magnetic separation, collecting the precipitate at the bottom of the polyethylene bottle after about 4s, removing the supernatant to obtain precipitate, washing the precipitate with distilled water, performing magnetic separation with magnet, repeating the above steps until precipitate without chloride is obtained, oven drying the precipitate at 100 deg.C, and grinding to obtain nanometer α -Fe2O3。
Rice-grain α -Fe2O3The electron micrograph is shown in FIG. 7 (α -Fe2O3As a mixed powder), synthesized nano-Fe2O3Is α -Fe2O3Crystal form and high purity; the synthesized nano-particles are rice-grain-shaped nano-particles, and have good monodispersity and good magnetism, the magnetic separation process is about 5s, and the recovery rate reaches more than 99%.
Cytotoxicity test:
taking a proper amount of nano-materials synthesized by the method of the invention, exposing rat kidney cells to 100mg/L of each nano-material for 12 hours, and selecting the concentrationBecause this concentration is much higher than the ambient concentration of such nanomaterials and the concentration of common biological imaging agents or targeted drug delivery. And (3) detecting the cell activity before and after exposure by using a WST-1 cell activity detection kit, and determining the cytotoxicity. As shown in FIG. 8, the cell activity and the nano Fe content of the control sample are shown from left to right3O4Exposed cellular Activity, granular α -Fe2O3Cellular viability under exposure and rice-grain α -Fe2O3The cell activity of the exposed nano material, as can be seen from fig. 8, the high concentration of the nano material has no significant toxic effect on the cell activity. The nano materials have good biocompatibility and are environment-friendly, and can be applied to environmental protection, medicines and bioengineering.
Claims (9)
1. A synthesis device of iron oxide magnetic nano materials is characterized by comprising a three-neck round-bottom flask (6), a water bath (10), a constant-temperature magnetic stirrer (11), a vacuum pump (1) and an air bag (2), wherein the water bath (10) is placed on a supporting plate of the constant-temperature magnetic stirrer (11), water (10a) is filled in a cavity of the water bath (10), the lower part of the three-neck round-bottom flask (6) is soaked in the water, an air inlet of the vacuum pump (1) is connected with a first interface of a tee joint (5) through a first hose (3a), an air outlet of the air bag (2) is connected with a second interface of the tee joint (5) through a second hose (3b), a third interface of the tee joint is connected with one inlet and outlet of the three-neck round-bottom flask (6) in a sealing manner through a third hose (3c), and a burette (8) and a separating funnel (9) which are connected in a sealing manner are respectively arranged on the other two inlets and outlets of the three-neck flask, a first valve (4a) is arranged on the first hose (3a), a second valve (4b) is arranged on the second hose (3b), and a third valve (4c) is arranged on the third hose (3 c).
2. The device for synthesizing the iron oxide magnetic nanomaterial according to claim 1, wherein rubber stoppers (62) are respectively mounted at three inlets and outlets (61) of the three-necked round-bottomed flask (6), a feeding channel (62a) which is through from top to bottom is formed in the center of each rubber stopper (62), and the discharge ends of the burette (8) and the separating funnel (9) are placed in the feeding channel (62a) and tightly attached to the inner wall of each rubber stopper to form a sealed feeding structure of the three-necked round-bottomed flask.
3. The synthesis apparatus of iron oxide magnetic nanomaterial according to claim 2, wherein the end of the third hose (3c) that is hermetically connected to the inlet and outlet of the three-necked round-bottomed flask (6) is equipped with a connector insert tube (7), and the discharge end of the connector insert tube (7) is placed in the feed channel (62a) and tightly attached to the inner wall of the rubber stopper to form a sealed gas inlet and outlet channel structure of the three-necked round-bottomed flask.
4. The synthesis device of iron oxide magnetic nanomaterial according to claim 1, wherein the thermostatic magnetic stirrer (11) is placed on a workbench (17), the workbench (17) is further provided with a positioning bracket (15), and the positioning bracket is provided with a fixing clamp (16) for fixing the positions of the three-neck round-bottom flask (6), the burette (8) and the separating funnel (9).
5. The synthesis device of iron oxide magnetic nano material according to claim 4, characterized in that the working table (17) is further provided with a drying and collecting device for drying and collecting iron oxide magnetic nano material, wherein the drying and collecting device comprises a polyethylene bottle (12), a magnet (13) and a constant temperature drying oven (14).
6. The apparatus for synthesizing iron oxide magnetic nanomaterial according to claim 1, wherein the gas bag (2) is filled with an inert gas as nano Fe3O4The protective gas or the air bag of the synthetic reaction is filled with high-purity oxygen which is used as nanometer α -Fe2O3Protective gas for the synthesis reaction.
7. The synthesis plant of iron oxide magnetic nanomaterials of claim 1, wherein the water bath (10) is provided with a thermometer (18) for monitoring the water temperature.
8. Nano Fe using the synthesis device of claim 13O4The synthesis method is characterized by comprising the following steps:
(1) nano Fe3O4Synthesis of (2)
Closing the first valve (4a), the second valve (4b) and the third valve (4c), connecting the gas bag filled with inert gas with the second hose (3b), dissolving ferrous salt and ferric salt with ultrapure water to obtain a mixed solution, wherein Fe in the mixed solution2+And Fe3+The molar ratio of (1: 2), adding the mixed solution into a separating funnel (9), closing a valve (9a) of the separating funnel (9), hermetically connecting an outlet of the separating funnel (9) with one inlet and outlet of a three-neck round-bottom flask (6), adding an alkaline liquid into a burette, closing a valve (8a) of the burette (8), hermetically connecting an outlet of the burette with the other inlet and outlet of the three-neck round-bottom flask (6), opening the valve (9a) of the separating funnel (9), adding the mixed solution in the separating funnel (9) into the three-neck round-bottom flask (6), closing the valve (9a) of the separating funnel (9), hermetically connecting a third hose with the last inlet and outlet of the three-neck round-bottom flask (6), opening a first valve (4a) and a third valve (4c) when the three-neck round-bottom flask (6) is in a relatively closed environment, the first hose and the third hose are communicated, the second hose is closed, the vacuum pump (1) is started, air in the three-neck round-bottom flask (6) is exhausted until the pump pressure of the vacuum pump is not changed any more, the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, the first valve (4a) is closed, the second valve (4b) is opened, the second hose and the third hose are communicated, the first hose is closed, the inner cavity of the three-neck round-bottom flask is automatically filled with inert gas through the second hose and the third hose under the action of the negative pressure of the inert gas in the gas bag, the third valve (3c) is closed when the volume of the gas bag is not changed any more, and at the moment, the reaction space in the three-neck round-bottom flask is filled with the inert gas, and the reaction process is guaranteed to be;
opening the constant temperature magnetic stirrer (11), adjusting the temperature of the constant temperature magnetic stirrer (11), heating the mixed liquid to 80 ℃ through the water constant temperature water bath in the water bath (10), opening the rotor of the constant temperature magnetic stirrer (11) to stir continuously, andopening a valve (8a) of the burette (8), adding alkaline liquid, controlling the pH value of the mixed solution between 8.0 and 14, reacting at constant temperature for about 40min, completing the reaction, and cooling to obtain Fe3O4A nanoparticle suspension;
(2) cleaning, drying and collecting
Fe to be synthesized3O4Carrying out magnetic separation on the nanoparticle suspension, and removing the supernatant to obtain a precipitate; then washing the precipitate with methanol and ultrapure water respectively until the pH of the precipitate is neutral, and drying the precipitate to obtain the nano Fe3O4。
9. Nano α -Fe using the synthesis device of claim 12O3The synthesis method is characterized by comprising the following steps:
(1) nanometer α -Fe2O3Synthesis of (2)
Closing the first valve (4a), the second valve (4b) and the third valve (4c), connecting a gas bag filled with high purity oxygen with a second hose (3b), adding pure water or a trivalent iron salt solution into the three-neck round-bottom flask through the inlet and outlet of the three-neck round-bottom flask (6), adding the trivalent iron salt solution into a separating funnel (9), closing the valve (9a) of the separating funnel (9), hermetically connecting the outlet of the separating funnel (9) with one inlet and outlet of the three-neck round-bottom flask (6), adding concentrated hydrochloric acid into the burette, closing the valve (8a) of the burette (8), hermetically connecting the outlet of the burette with the other inlet and outlet of the three-neck round-bottom flask (6), hermetically connecting the third hose with the last inlet and outlet of the three-neck round-bottom flask (6), and at the moment, placing the three-neck round-bottom flask (6) in a relatively closed environment, opening a first valve (4a) and a third valve (4c) to enable the first hose and the third hose to be communicated, closing a second hose, opening a vacuum pump (1) to exhaust air in the three-neck round-bottom flask (6) until the pump pressure of the vacuum pump is not changed any more, indicating that the first hose, the third hose and the three-neck round-bottom flask are in a vacuum state, closing the first valve (4a), opening a second valve (4b) to enable the second hose and the third hose to be communicated, sealing the first hose, automatically filling the inner cavity of the three-neck round-bottom flask through the second hose and the third hose under the action of negative pressure of high-purity oxygen in the air bag, closing the third valve (3c) when the volume of the air bag is not changed any more, and ensuring that the reaction process is finished under the high-purity oxygen environment;
opening a constant-temperature magnetic stirrer (11), adjusting the temperature of the constant-temperature magnetic stirrer (11), heating pure water or a trivalent ferric salt solution in a three-neck round-bottom flask to 90-100 ℃ through a water constant-temperature water bath in a water bath (10), opening a valve (8a) of a burette (8), adding concentrated hydrochloric acid, opening a rotor of the constant-temperature magnetic stirrer (11) to stir continuously, opening a valve (9a) of a separating funnel (9) simultaneously, adding the trivalent ferric salt solution, and enabling Fe in the three-neck round-bottom flask to be in Fe state3+The molar concentration ratio of the solution to hydrochloric acid is 2:1-10:1, the pH value is controlled to be 1.0-3.0, a valve (8a) of a burette (8) and a valve (9a) of a separating funnel (9) are closed, stirring is carried out until the trivalent ferric salt is completely dissolved, then a sealed three-neck round-bottom flask is placed into a constant temperature drying box (14) with the temperature of 100 ℃, the constant temperature is kept for 24-48 h, and then the synthesis is finished to obtain α -Fe2O3A nanoparticle suspension;
(2) cleaning, drying and collecting
The synthesized α -Fe2O3Magnetically separating the suspension of nanoparticles, removing the supernatant to obtain precipitate, repeatedly washing the precipitate with distilled water until chloride-free precipitate is obtained, and drying to obtain α -Fe nanoparticles2O3。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111774008A (en) * | 2020-07-07 | 2020-10-16 | 烟台大学 | Online constant-temperature oxygen-free solution synthesis reaction device and method |
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| CN117504797A (en) * | 2023-12-29 | 2024-02-06 | 常州新一产生命科技有限公司 | Synthetic column structure and biochemical reaction equipment |
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